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the coking properties of coal at elevated pressures. - Argonne ...

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L<br />

Table I: Compositions <strong>of</strong> High Temper<strong>at</strong>ure Ash (HTA)<br />

Coal Name<br />

Coal Rank<br />

%H TA<br />

Si02(%a)***<br />

A120 (%a)<br />

Ti 023%a)<br />

Fe 20 3( %a )<br />

MgO (%a)<br />

CaO( %a)<br />

Na20( %a)<br />

K20(%a)<br />

P205(%a)<br />

s03( %a)<br />

Trace Elements<br />

>1000ppm <strong>of</strong> HTA<br />

(in ppm <strong>of</strong> HTA)<br />

Hagel Seam*<br />

Lignite<br />

9.66<br />

28,20<br />

9.35<br />

0.58<br />

8.20<br />

5,91<br />

24 50<br />

2.81<br />

0.33<br />

0.10<br />

17.40<br />

Ba-6700<br />

Sr-3150<br />

Cumber1 and Fuel **<br />

High Vol<strong>at</strong>ile<br />

Bituminous<br />

18.8<br />

51 .3<br />

19.8<br />

002<br />

17.0<br />

1.2<br />

4.9<br />

oo9<br />

2.8<br />

0.2<br />

1.6<br />

Not<br />

Available<br />

Pennsylvania<br />

#2 Seam*<br />

Semianthracite<br />

30.74<br />

80 .OO<br />

12,lO<br />

3.09<br />

1.47<br />

0.05<br />

0.30<br />

0.05<br />

0-35<br />

0,05<br />

0,30<br />

None<br />

Reported<br />

"Inform<strong>at</strong>ion courtesy <strong>of</strong> <strong>the</strong> Penn St<strong>at</strong>e Coal D<strong>at</strong>a Base<br />

**Inform<strong>at</strong>ion taken from reference (8).<br />

***%a - oxide % <strong>of</strong> HTA <strong>of</strong> dry <strong>coal</strong><br />

Experimental Procedure<br />

The STEM used in <strong>the</strong> present study was a JOEL 200CX equipped with a Tracor-<br />

Nor<strong>the</strong>rn T!42000 energy dispersive spectrometry (EDS) system for x-ray analysis<br />

The fe<strong>at</strong>ures <strong>of</strong> STEM oper<strong>at</strong>ion pertinent to this work are illustr<strong>at</strong>ed in Figure 1,<br />

The sample was illumin<strong>at</strong>ed by a narrow probe <strong>of</strong> 200kV electrons which was scanned<br />

across its surface. Transmitted electrons were used to form an image <strong>of</strong> <strong>the</strong> sample<br />

volume being scanned, The probe could also be stopped and fixed on some fe<strong>at</strong>ure<br />

<strong>of</strong> interest in <strong>the</strong> sample, <strong>at</strong> which point <strong>the</strong> characteristic x-rays emitted by <strong>the</strong><br />

<strong>at</strong>oms under <strong>the</strong> probe could be analyzed to obtain chemical inform<strong>at</strong>ion from a<br />

sample region with a diameter approaching th<strong>at</strong> <strong>of</strong> <strong>the</strong> probe diameter. Chemical<br />

characteriz<strong>at</strong>ion could be accomplished in this manner for all elements with <strong>at</strong>omic<br />

number 2211<br />

For studies <strong>of</strong> mineral m<strong>at</strong>ter embedded in particles <strong>of</strong> powdered <strong>coal</strong>, advan-<br />

tage was taken <strong>of</strong> <strong>the</strong> difference in image contrast between <strong>the</strong> crystalline<br />

mineral particles and <strong>the</strong> surrounding amorphous organic m<strong>at</strong>rix. The crystalline<br />

particles are capable <strong>of</strong> diffracting electrons, and so appeared in strong contrast<br />

when held <strong>at</strong> specific angles to <strong>the</strong> incident electron beam.<br />

needed only to be tilted through some moder<strong>at</strong>e range <strong>of</strong> angles (generally + 45"<br />

from <strong>the</strong> horizontal) to quickly establish <strong>the</strong> loc<strong>at</strong>ions <strong>of</strong> <strong>the</strong> minerals wiThin<br />

a given <strong>coal</strong> particle. During <strong>the</strong> tilting such particles abruptly "winked" in and<br />

out <strong>of</strong> strong diffractiDn contrast, while <strong>the</strong> amorphous m<strong>at</strong>rix changed contrast<br />

only gradually as a function <strong>of</strong> <strong>the</strong> change in sample thickness intercepted by<br />

<strong>the</strong> electron beam. An example <strong>of</strong> an image <strong>of</strong> a mineral particle visible by strong<br />

diffraction contrast amidst an amorphous <strong>coal</strong> m<strong>at</strong>rix is shown in Figure 2,<br />

estim<strong>at</strong>ed th<strong>at</strong> <strong>the</strong> imaging procedure could detect mineral particles with diameters<br />

>-2nm. Particles smaller than this would most likely remain indistinguishable<br />

from <strong>the</strong> amorphous m<strong>at</strong>rix,<br />

llith <strong>the</strong> loc<strong>at</strong>ion <strong>of</strong> an embedded mineral particle thus determined, <strong>the</strong> probe<br />

was fixed on <strong>the</strong> mineral and an x-ray spectrum was acquired, Except in <strong>the</strong> instance<br />

where <strong>the</strong> mineral extended through <strong>the</strong> full thickness <strong>of</strong> <strong>the</strong> <strong>coal</strong> particle<br />

intercepted by <strong>the</strong> probe, this spectrum consisted <strong>of</strong> a superposition <strong>of</strong> a particle<br />

spectrum and a m<strong>at</strong>rix spectrum.<br />

The sample thus<br />

To determine <strong>the</strong> signal associ<strong>at</strong>ed with <strong>the</strong><br />

It is<br />

inclusion, <strong>the</strong> probe was subsequently moved 1-2 particle diameters away to a region<br />

<strong>of</strong> <strong>the</strong> m<strong>at</strong>rix known to be free <strong>of</strong> o<strong>the</strong>r minerals (within <strong>the</strong> resolution limit<strong>at</strong>ion<br />

125

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